Indian Journal of Chemical Technology


Total visitors:2,182 since 14-9-05

 

Volume 12

Number 5

SEPTEMBER 2005

CODEN:ICHTEU 12(5) 507-620

 

ISSN:0971-457X

 

CONTENTS

 

Research articles

 

 

 

Removal and recovery of nitrate from water by ZnCl2 activated carbon from coconut coir pith, an agricultural solid waste

 

513

        IPC Code: C02F1/28

 

        C Namasivayam & D Sangeetha

 

 

 

Removal of mercury(II) ions by adsorption onto dates nut and commercial activated carbons: A comparative study

 

522

        IPC Code: C02F3/00; C01B31/00; C02F101:30

 

        N Kannan & S Jasmin Sugantha Malar

 

 

 

Preservation of bagasse using microbial growth / enzyme inhibitors as biotech preservatives

528

        IPC Code: B27K9/00

 

        K R Yadav, R P Patil, A B Chaudhari, R K Sharma & R M Kothari

 

 

 

Studies on chemical analogy of calcium and beryllium in soil

534

        IPC Code: C09K17/06

 

        P N Bhat, S Soundararajan & D K Ghosh

 

 

 

Preparation of reusable enzyme strip for determination of serum triglyceride

539

        IPC Code: A61K38/43

 

        Minakshi & C S Pundir

 

 

 

Four rapid and sensitive methods for the assay of amoxycillin in pharmaceuticals using bromate-bromide mixture and two dyes

 

543

        IPC Code: A61K9/00

 

        V Ramakrishna & K Basavaiah

 

 

 

Effect of some commercial flocculating agents on settling and filtration rates of low grade, fragile manganese ores of Andhra Pradesh

 

550

        IPC Code: C02F1/52

 

        S B Kanungo

 

 

 

Study of water vapour adsorption on nickel-chromia H-D exchange catalyst

559

        IPC Code: B01D15/00

 

        J S Gill, P Ramakrishnan & H Singh

 

 

 

Kinetic determination of mercury(II) at trace level from its catalytic effect on ligand substitution reaction between hexacyanoferrate(II) and nitroso-R-salt

 

563

        IPC Code: C22B43/00

 

        R M Naik & Joy Sarkar

 

Role of corrosion inhibitor on bacterial corrosion in petroleum product pipelines

567

        IPC Code: C12S1/100; C23F11/00

 

        S Maruthamuthu, S Mohanan, A Rajasekar, N Muthukumar, S Ponmarippan,
P Subramanian & N Palaniswamy

 

 

 

Thiadiazoles-A potential class of heterocyclic inhibitors for prevention of mild steel corrosion in hydrochloric acid solution

 

576

        IPC Code: C23F11/00

 

        M A Quraishi & S Khan

 

 

 

Magnetic and processability studies of nitrile rubber vulcanisates containing barium ferrite and carbon black

 

582

        IPC Code: C08C4/00; 19/00

 

        M A Soloman, Philip Kurian, M R Anantharaman & P A Joy

 

 

 

Notes

 

 

An ultrasonic study of multicomponent liquid systems

588

        IPC Code: B01J19/10

 

        J D Pandey, A K Singh & Ranjan Dey

 

 

 

Spectrophotometric determination of dissolved oxygen in water

593

        IPC Code: G01J3/00

 

        B Narayana, Mendalin Mathew, Tom Cherian & Chand Pasha

 

 

 

Spectrophotometric determination of chromium using saccharin

596

        IPC Code: G01J3/00

 

        Tom Cherian & B Narayana

 

 

 

Educator

 

 

Platinum -From exotic to commodity

601

        Jaime Wisniak

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 513-521

 

Removal and recovery of nitrate from water by ZnCl2 activated carbon from coconut coir pith, an agricultural solid waste

 

C Namasivayam* & D Sangeetha

Nitrate removal from aqueous solution was investigated using ZnCl2 activated carbon developed from coir pith. Influence of contact time, adsorbent dose, nitrate concentration, pH and temperature were investigated. Two theoretical adsorption isotherms namely Langmuir and Freundlich were used to describe the experimental results. The Langmuir adsorption capacity (Qo) was found to be 10.3 mg nitrate per g of the adsorbent. Adsorption followed second order kinetics. Adsorption was maximum in the pH range 3-10. pH effect and desorption studies showed that ion exchange mechanism might be involved in the adsorption process. Effects of foreign ions such as chloride, sulphate, phosphate and perchlorate on the removal of nitrate have also been investigated. Removal of nitrate from ground water was also tested. Results show that ZnCl2 activated coir pith carbon is effective for the removal of nitrate from water.

 

Keywords: Coir pith, ZnCl2 activated carbon, nitrate, adsorption isotherms

IPC Code: C02F1/28

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 522-527

 

Removal of mercury(II) ions by adsorption onto dates nut and commercial activated carbons: A comparative study

N Kannan* & S Jasmin Sugantha Malar

Studies on the removal of mercury(II) ions by adsorption onto indigenously prepared dates nut (DC) and commercial activated carbons (CAC) have been carried out with an aim to obtain data for treating effluents from metal processing and chloralkali industries. The effect of various process parameters has been investigated by following the batch adsorption technique at 30±1 ºC. The percentage removal of mercury(II) ions increased with the decrease in initial concentration and increase in contact time and dose of adsorbent. As initial pH of the slurry increased, the percentage removal increased and reached a maximum value. The process parameters were optimised. Adsorption data were modeled  with the Freundlich and Langmuir isotherms, the first order kinetic equations proposed by Lagergren and Bhatacharya and Venkobachar and Weber-Morri’s intra-particle diffusion model and the equations models were found to be applicable. The kinetics of adsorption is observed to be first order with intra-particle diffusion as one of the rate determining steps. Removal of mercury(II) ions by DC and CAC is found to be favourable and hence DC could be employed as an alternative low-cost adsorbent for effluent treatment, especially for the removal of mercury(II) and other metal ions.

Keywords: Mercury(II), activated carbon, dates nut carbon, adsorption, kinetic equations, intra-particle diffusion

IPC Code: C02F3/00; C01B31/00; C02F101:30

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 528-533

 

Preservation of bagasse using microbial growth/enzyme inhibitors as biotech preservatives

K R Yadav, R P Patila, A B Chaudharia, R K Sharma & R M Kotharib*

Exposure of bagasse to 4 biotech preservatives such as neembicide, multicide, copper sulphate and celphos (reference standard) was explored for its preservation at 200 kg scale for 6 months under ambient conditions, mimicking pulp and paper mill practices. Bacterial and fungal count, temperature and pH, reducing sugars and soluble content, fibre and pith content and cellulose/hemi-cellulose were monitored at a monthly frequency to judge the efficacy of the above preservatives. Among them, neembicide appeared to be superior to others, besides being cost-effective by virtue of superior fibre/cellulose protection, it is eco-friendly by virtue of being biodegradable and operationally practical preservative on the basis of parameters monitored. Its application is suggested for large scale trials.

Keywords: Bagasse, preservation, biotech preservatives, eco-friendly preservative, cost-effective preservation

IPC Code: B27K9/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 534-538

 

Studies on chemical analogy of calcium and beryllium in soil

P N Bhat*, S  Soundararajan & D K Ghosh 


This study was specifically aimed to determine the levels of beryllium and calcium in the soil collected near the vicinity of a beryllium processing facility (BPF) and to assess the effect of calcium addition, if any, to the soil. Atomic Absorption Spectrophotometer (AAS) technique was used to estimate the total beryllium and calcium.  The beryllium and calcium contents per gram of soil samples were in the range of  0.8-3.02  and 1150-22535 µg respectively. The loading of collected samples with salts of calcium revealed analogy with beryllium. This was supported by the rejection of beryllium by calcium-loaded soils. 

Keywords: Beryllium, calcium, chemical analogy

IPC Code: C09K17/06

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 539-542

 

Preparation of reusable enzyme strip for determination of serum triglyceride

Minakshi & C S Pundir

 

Lipase, glycerol kinase (GK), glycerol-3-phosphate oxidase and peroxidase were co-immobilized onto alkylamine glass beads affixed on a plastic strip with a conjugation yield of 80.0 mg/g support and 57.41% retention of specific activity. The enzyme showed an increase in optimum pH, incubation temperature, energy of activation and time of incubation, but decrease in Km and Vmax. A method for determination of serum triglycerides was developed, employing strip bound enzymes. The minimum detection limit of the method was 0.61 mM/L. The recovery of added triglycerides was 82.2%. Within and between assay coefficient of variation were < 3.1 and < 14.2 respectively. A good correlation (r=0.973) was found between triglycerides value obtained by commercial enzymatic colourimetric method and present method. The strip provided 100 reuses of co-immobilized enzymes with ease.

Keywords: Triglycerides, lipase, GK, GPO, peroxidase, alkylamine glass bead, plastic strip, co-immobilization

IPC Code: A61K38/43

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 543-549

 

 

Four rapid and sensitive methods for the assay of amoxycillin in pharmaceuticals using bromate-bromide mixture and two dyes

V Ramakrishna  & K Basavaiah

 

Four new methods using titrimetry and spectrophotometry are described for the rapid determination of amoxycillin in bulk drug and dosage forms. In direct titrimetry (Method A), the drug is titrated with bromate–bromide mixture in acid medium using methyl orange indicator. Back titrimetry (Method B) entails adding a known excess amount of bromate-bromide mixture to the drug solution in acid medium, followed by determination of residual bromine iodometrically. Both spectrophotometric methods are based on the oxidation–bromination of amoxyciillin by in situ generated bromine followed by estimation of unreacted bromine with methyl orange (Method C) or indigo carmine (Method D) and measuring the change in absorbance at 520 or 610 nm. In all the methods, qunatitation is based on the amount of bromate that has reacted with amoxycillin. The experimental conditions have been optimized. Calculations are based on 1:1 and 1:2 (amoxycillin: bromate) stoichiometry for method A and Method B, respectively. Method A is applicable over 2-16 mg range, and 1-9 mg of amoxycillin could be determined by method B. In spectrophotometric methods, the absorbance is found to increase linearly with increasing concentration of amoxycillin which is corroborated by the calculated correlation coefficient (r) of 0.9964 (Method C) and 0.9959 (Method D). The calibration graphs are found to be linear over 0.1–1.2 and 0.5 – 4.0 mg mL-1 for method C and method D, respectively. Method C with a molar absorptivity of 1.60 ´ 105 L mol-1 cm-1 is found to be more sensitive than method D (ε = 5.83 ´ 104 L mol-1 cm-1). The limits of detection and quantification for both spectrophotometric methods are reported. Statistical evaluation of the methods was examined by determining intra-day and inter-day precisions. The methods were applied to the determination of amoxycillin pharmaceutical formulations. No interference was observed from excipients and the validity of the methods was tested against a reference method.

Keywords: Amoxycillin determination, titrimetry, spectrophotometry, bromate-bromide, dyes

IPC Code: A61K9/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 550-558

 

 

Effect of some commercial flocculating agents on settling and filtration rates
of low grade, fragile manganese ores of Andhra Pradesh

 

S B Kanungo

The highly weathered, fragile and low grade manganese ores of Visakhapatnam district of Andhra Pradesh are subjected to wet high intensity magnetic separation (WHIMS) to give beneficiated magnetic fraction. However, the original ore and its non-magnetic fraction contain large quantities of slimy particles which are difficult to separate from their aqueous suspensions. Three different commercial flocculating agents with anionic, cationic and non-ionic characters have been used to improve settling and filtration behaviour of the suspensions. While a small dose of anionic flocculant has been found to be very effective, cationic flocculant is poorly effective even at high dosage. The behaviour of non-ionic flocculant is intermediate between the two. Since extremely fine particles constitute the non-magnetic fraction, it needs higher dosage of anionic flocculant to form large or aggregated flocs which make the filter cake porous even with increasing slurry concentration.

Keywords: Manganese ore fines, flocculation, polymeric flocculants, settling and filtration rates, specific cake resistance

IPC Code: C02F1/52

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 559-562

 

 

Study of water vapour adsorption on nickel-chromia H-D exchange catalyst

 

J S Gill, P Ramakrishnan & H Singh


Adsorption of water vapour on a series of nickel-chromia samples has been studied. Nickel-chromia, with 15% chromium is an active catalyst for H-D (hydrogen-deuterium) exchange in hydrogen-water system, where water is in vapour phase. Water vapour adsorption/desorption indicate that it is adsorbed on the catalyst both physically and chemically. The 15% chromium catalyst sample has been treated with phenylethyl triethoxy silane to make it hydrophobic and active in liquid water-hydrogen system of H-D exchange. Water vapour adsorption isotherm on the treated sample shows the hydrophobization of the catalyst.

Keywords: Vapour adsorption, nickel-chromia catalyst, H-D exchange, phenylethyl triethoxy silane

IPC code: B01D15/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 563-566

 

 

Kinetic determination of mercury(II) at trace level from its catalytic effect on ligand substitution reaction between hexacyanoferrate(II) and nitroso-R-salt

R M Naik  & Joy Sarkar


A kinetic method is described for the determination of mercury(II), based on its catalytic effect on the ligand substitution reaction between hexacynoferrate(II) and Nitroso-R-Salt. The reaction is followed spectrophotometrically by measuring the absorbance at fixed times at 720 nm, the λmax of green coloured complex, [Fe(CN)5NRS]3– formed during the course of reaction under optimum reaction conditions viz, temp = 25.0±0.1
°C, pH = 6.5±0.02 and I = 0.1 M(KNO3). The method is simple, sensitive, selective, rapid and allows the determination of as little as 10–6 M of mercury with good accuracy and precision. The detection limit is computed by standard procedure and found to be 1.6 ´ 10–7 M of [Hg2+]. The effects of few interfering and non-interfering cations and anions on mercury(II) determination have also been reported with relative standard deviations.

Keywords: Mercury(II) determination, Kinetics, ligand substitution reaction, hexacyanoferrate(II), nitroso-R-salt

IPC Code: C22B43/00

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 567-575

 

 

Role of corrosion inhibitor on bacterial corrosion in petroleum product pipelines

S Maruthamuthu, S Mohanan, A Rajasekar, N Muthukumar,

S Ponmarippan, P Subramanian & N Palaniswamy


Petroleum product pipelines in India are found to contain a large number of various types of microorganisms either aerobic or anaerobic and these microorganisms either directly or indirectly enhance corrosion. Field studies have been carried out by CECRI to investigate the corrosion problem in a cross-country pipeline transporting petroleum product (diesel) for about 1400 km. Heterotrophic bacteria, iron bacteria, manganese oxidizers, acid producers were enumerated and identified in the pipeline whereas SRB could not be noticed in the pipeline. The reason for the absence of SRB is explained in the present study. Moreover, the interaction between heterotrophic and chemolithotrophic bacteria is explained with FTIR and NMR analysis. Influence of inhibitor on microbial corrosion has been investigated and the importance of selection of inhibitor has also been explained.

Keywords: Sulphate reducing bacteria, microbial corrosion, degradation, FTIR, NMR, XRD

IPC Code: C12S1/100; C23F11/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 576-581

 

 

Thiadiazoles-A potential class of heterocyclic inhibitors for prevention of mild steel corrosion in hydrochloric acid solution

 

M A Quraishi & S Khan


Four organic inhibitors namely 2-amino-1,3,4-thiadiazole (AT), 5-methyl-2-amino-1,3,4-thiadiazole (MAT), 5-ethyl-2-amino-1,3,4-thiadiazole (EAT) and 5-propyl-2-amino-1,3,4-thiadiazole (PAT) were synthesized and their influence on the inhibition of corrosion of mild steel (MS) in hydrochloric acid was investigated by weight loss and potentiodynamic polarization techniques. The inhibition efficiency (IE) of these compounds was found to vary with the inhibitor concentration, immersion time, acid concentration and solution temperature. All the investigated thiadiazoles exhibited good inhibition efficiency (IE) for mild steel in hydrochloric acid solution. The adsorption of all these compounds on mild steel in acid solution has been found to obey Langmuir’s adsorption isotherm. The potentiodynamic polarization data showed that the inhibitors are of mixed type. Various thermodynamic parameters (Ea, ΔGads, ΔQ, ΔH, ΔS, t1/2) have also been calculated to investigate the mechanism of corrosion inhibition.

Keywords: Corrosion inhibition, thiadiazoles, mild steel, potentiodynamic polarization, langmuir adsorption isotherm

IPC Code: C23F11/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 582-587

 

Magnetic and processability studies of nitrile rubber vulcanisates containing barium ferrite and carbon black

M A Soloman, Philip Kurian, M R Anantharamanc & P A Joy


Fine particles of barium ferrite (BaFe12O19) belonging to the M-type hexagonal ferrites were prepared by the conventional ceramic techniques. They were incorporated into a nitrile rubber matrix according to a specific recipe for various loadings to produce rubber ferrite composites (RFC). The percolation threshold is not reached for a maximum loading of 130 phr (parts per hundred rubber). Here in this paper, the magnetic properties and processability of the nitrile rubber based RFCs containing barium ferrite (BaF) and HAF carbon black is reported. The magnetic properties of the ceramic ferrite and these rubber ferrite composites were evaluated and it was found that the coercivity values of RFCs were less than that of the ceramic BaF, but remained constant with the loading of both the ferrite filler and carbon black. However, other properties like saturation magnetization and magnetic remanence increased with the loading of ferrite filler.

Keywords: Magnetic materials, barium ferrite, rubber ferrite composites, nitrile rubber, carbon black

IPC Code: C08C4/00; 19/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September. 2005, pp. 588-592

 

 

An ultrasonic study of multicomponent liquid systems

J D Pandey, A K Singh & Ranjan Dey


A modified Flory theory has been employed for the computation of ultrasonic velocity of four quaternary liquid mixtures at 298.15 K. Ultrasonic velocity of these four systems have also been computed using Van Dael ideal mixing relation, Nomoto relation and Collision factor theory. A comparative study has then been carried out as regards the merits and demerits of the employed relations.

Keywords: Quaternary liquid mixtures, ultrasonic velocity, Flory theory

IPC Code: B01J19/10

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 593-595

 

 

Spectrophotometric determination of dissolved oxygen in water

B Narayana, Mendalin Mathew, Tom Cherian & Chand Pasha


A simple, rapid and sensitive spectrophotometric method has been developed for the determination of dissolved oxygen (DO) in river water samples. The method is based on the reaction of dissolved oxygen with manganous sulphate in alkaline iodide-azide solution and the liberation of iodine by manganese dioxide. The liberated iodine bleaches the violet colour of azure B which is measured at 644 nm. The decrease in absorbance is directly proportional to dissolved oxygen concentration and obeys Beer’s law in the range 0.2-1.4 mgmL-1. The molar absorptivity, Sandell’s sensitivity, detection limit and quantitation limit of the method were found to be 5.86 ´ 104 Lmol-1 cm-1, 3.66 ´ 10-3 mg/cm2, 0.030 and 0.090 mgmL-1, respectively.

 

Keywords:                     Dissolved oxygen determination, spectrophotometry,                    azure B

IPC Code: G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 596-600

 

 

Spectrophotometric determination of chromium using saccharin

 

Tom Cherian & B Narayana


A sensitive and selective spectrophotometric method for the indirect determination of trace amounts of chromium(VI) is described. Chromium(VI) oxidizes hydroxylamine in acetate buffer of pH 4.0 to nitrite, which then diazotizes p-nitroaniline or sulphanilamide to form diazonium salt. These diazonium salts are then coupled with saccharin in an alkaline medium, which gives azo dye with absorption maximum at 372 and 390 nm for p-nitroaniline and sulphanilamide, respectively. The method obeys Beer’s law in the concentration range of 1-16 mgmL-1 for chromium with p-nitroaniline-saccharin and 0.6-14 mgmL-1 of chromium with sulphanilamide-saccharin couples. The molar absorptivity, Sandell’s sensitivity of the systems with p-nitroaniline-saccharin and sulphanilamide-saccharin couples were found to be 5.41´104 Lmol-1cm-1, 1.93´10-3 mgcm-2 and 2.63´104 Lmol-1cm-1, 3.9´10-3 mgcm-2, respectively. The optimum reaction conditions and other analytical parameters were evaluated. The effect of interfering ions on the determination was described. Chromium(III) can be determined after it is oxidized with bromine water in an alkaline medium to chromium(VI). The developed method has been successfully applied to the analysis of the chromium in alloy steel, pharmaceutical samples, natural water and soil samples.

Keywords: Chromium determination, spectrophotometry,, p-nitroaniline, sulphanilamide, saccharin

IPC Code: G01J3/00

 

 

Indian Journal of Chemical Technology

Vol. 12, September 2005, pp. 601-614

 

 

Platinum ¾From exotic to commodity

Jaime Wisniak

 

Platinum was brought to Europe in the middle of the sixteenth century and was soon recognized a true metal, which could not be fused. It remained an expensive curiosity for almost 200 years, until scientists learned its properties, how to melt it in large quantity, and discovered that four new elements, rhodium, iridium, osmium, and palladium, accompanied it (the platinum group metals). The early uses of platinum were in jewelry, laboratory ware, and coin manufacture. By the end of the nineteenth century a platinum-rhodium alloy was adopted for constructing the standard meter and kilogram. Production of platinum grew very slowly; it was only about one ton per year by 1911. The breakthrough came with the discovery of the extraordinary the catalytic properties of the platinum metal group. Today these metals stand at the heart of the petrochemical industry and are the basis of all the means for controlling the emission of obnoxious gases of motor vehicles. Annual production has now reached near 190 tons.